食品科学 ›› 2016, Vol. 37 ›› Issue (20): 167-171.doi: 10.7506/spkx1002-6630-201620028

• 安全检测 • 上一篇    下一篇

离子交换高效液相色谱-串联质谱法测定鸡肉和鸡肝中的高氯酸盐

邵琳智,吴映璇,欧阳少伦,林 峰   

  1. 1.广东出入境检验检疫局检验检疫技术中心,广东 广州 510623;
    2.广东省动植物与食品进出口技术措施研究重点实验室,广东 广州 510623
  • 收稿日期:2016-10-27 修回日期:2016-10-27 出版日期:2016-10-25 发布日期:2016-12-01
  • 基金资助:

    国家认证认可监督管理委员会检验检疫行业标准计划项目(2009B535);广东检验检疫局科技计划项目(2015GDK10)

Determination of Perchlorate in Chicken Meat and Liver by Ion Exchange High Performance Liquid Chromatography-Tandem Mass Spectrometry

SHAO Linzhi, WU Yingxuan, OUYANG Shaolun, LIN Feng   

  1. 1. Inspection and Quarantine Technology Center, Guangdong Entry-Exit Inspection and Quarantine Bureau,
    Guangzhou 510623, China; 2. Key Laboratory of Animals and Plants and Food Import and Export of Technical Measures in
    Guangdong Province, Guangzhou 510623, China
  • Received:2016-10-27 Revised:2016-10-27 Online:2016-10-25 Published:2016-12-01

摘要:

建立测定鸡肉和鸡肝中高氯酸盐的离子交换高效液相色谱-串联质谱法。试样加18O标记高氯酸根离子后采用1%乙酸溶液-乙腈提取,固相萃取柱净化后,经IC-PakTM Anion HR (4.6 mm×75 mm ,6 μm)色谱柱分离,以乙腈-100 mmol/L乙酸铵溶液为流动相,采用电喷雾离子源串联质谱,在负离子扫描方式下以多反应监测模式检测,内标法定量。结果表明:高氯酸盐在0.2~10 μg/L质量浓度范围内线性关系良好,定量限为3.0 μg/kg。在3 个加标水平下的平均回收率为91.8%~96.0%,相对标准偏差为1.8%~6.5%。该方法操作简便、灵敏度高、抗干扰能力强、回收率和重复性良好,适用于鸡肉和鸡肝中高氯酸盐的测定。

关键词: 高氯酸盐, 同位素稀释技术, 固相萃取, 高效液相色谱-串联质谱, 鸡肉和鸡肝

Abstract:

A method was developed for the determination of perchlorate in chicken meat and liver by ion- exchange high
performance liquid chromatography-tandem mass spectrometry (IC-HPLC-MS/MS). After adding isotopically labeled
internal standards to it, the sample was extracted with 1% acetic acid-acetonitrile, and then purified by solid-phase extraction
column. The target compound was separated on an IC-PakTM Anion HR column (4.6 mm × 75 mm, 6 μm) using a mobile
phase consisting of acetonitrile and 100 mmol/L aqueous ammonium acetate, and detected by tandem mass spectrometry
in negative electrospray ionization and multiple reaction monitoring (MRM) mode. The quantification of perchlorate was
performed by the internal standard method. The calibration curves showed good linearity in the concentration range of
0.2–10 μg/L with a limit of quantification (LOQ) of 3.0 μg/kg. The recoveries in chicken meat and liver at three spiked levels
were in the range of 91.8%–96.0% with relative standard deviations (RSDs) between 1.8% and 6.5%. With the advantages
of convenience, high sensitivity, strong anti-interference capability and good recovery and repeatability, the method was
suitable for the analysis of perchlorate in chicken meat and liver.

Key words: perchlorate, isotope dilution technique, solid-phase extraction, high performance liquid chromatography-tandem mass spectrometry, chicken meat and liver

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